Process of making resin size.



m. 70|,|25 Patented May 27, I902.

F. a H. ABLEDTER. PROCESS OF MAKING RESIN SIZE.

(Application filed Jan. 25, 1902.) (N 0 M 0 1! e1.)

A TTOHNE VS F U ITED STATES,

PATENT OFFICE.

FRITZ ARLEDTER, on NEW, YORK, N. Y., AND HERMAN ARLEDTER, or

, GARSTON, ENGLANI) PROCESS OF'MAKING RESIN SIZE.-

SIEECIFICATION formingpart of Letters Patent No. 701,'l25, dated May 27, 1902.

Application filed January 25 1902.

, s'LEDTER', residing in Garston, England, subj ects of the Emperor of Austria-Hungary,have invented certain new and useful Improvements in Processes of Making Resin Size, of

.which the following is a specification..

This invention relates to processes of making resinsize, and in particular resin size suitable for use in the manufacture of paper. As is well known, the efiective agent of such a size is'the free or nnsaponified resin existing I inthe size and liberated within the paper during the course of manufacturing the same.

The object of this invention is' to provide a process for making a size containing a very high percentage of free resin and, furthermore, to provide a process by which a size containing free resin and a compound of resin-- in other words, a resinate-capable of decomposltion into; a volatile substance and free resin in the course of paper manufacture may '2 5 be obtained. The invention consists for this purpose in the process of making resin size, which comprises the steps of, mixing an oil or fat with a suitable molten resin, filtering the mixture, adding to the same a solution of an ammonium compound and an alkali lye, the

latter in suflicient quantity to induce saponification, and agitating the resulting mixture in contact with carbonic-acid gasunder conditions permitting saponification of only a part of the resin and the invention consists,

further, of a resin size containing free unsaponified resin, free alkali, and an ammonium resinate.

In the accompanying drawing, which illuso trates in. side elevation and partly in vertical section an apparatus suitable for carrying on our improved process, A indicates a suitable boiling vessel, which may be heated in any suitable manner-for example, by means of the heating-coil a.

F is a filter of suitable construction for filtering a mixture of molten resin and oil-and is connected by the pipe f with the boiler A.

13 indicates a cooker communicating at its 5o upper portion by a pipe b with the filter]? and provided with a manhole which is Serial No. 91,200. (No specimensr closed by a suitable cover, and with a ventcock b at the upper portion of the cooker. In

order to secure thorough heating of the mass treated within the cooker, the same is preferably heated both exteriorly and interiorly, exteriorl'y by means of a jacketb and interiorly by means of a steam-coil b. The latter is located at the lower portion of the cooker and immediately above a screen C, which divides the cooker laterally into two compartments,an upper and a lower one. From the lower compartment B a pipe d communicates with a filter F from which apipe'd extends to asuitable force-pump P. From said pump a pipe cl communicates with the upper com-- partment B A branch pipe d is connected at its lower end with the pipe d and at its opposite end with a pump P, and a pipe d delivers from the pump P into a suitable settling-vat D.

The various parts of the apparatus may be,

supported in any suitable manner, and the various pipes are provided with the necessary valves for carrying out the function of the apparatus- A quantity of resin is introduced into the boiler A. To the same is added a quantity of oil or fat, either mineral oil-for example, naphtha,or a vegetable oil-for example,

palm-oil. The quantity of oil'added is in pro- .j I.

portion to the quantity of resinand to the na- I ture of the resin and oil employed. The mass is heated to such an extent as to melt the resin,.whereby the same dissolves in the oil or fat, the whole forming a liquid 1nass,which is then allowed to run through the pipe f, filter F, and pipe b into the upper compartment B of the cooker B. Prior to the admission of this mass into the cooker, however, a quantity of alkali lye has been admitted through the manhole at theupper'part of the, cooker sufiicient to partly fill the lower compare ment B. i The lye is employed in approxi-' mately the proportion of six per cent. of the weight of the resin. Sodium carbonate 1s a suitable alkali for the purpose. There is also admitted a solution containmg about one per ture-is run in on top of them, the same pass- I ing through. the screen C. The pump P is now started, and the alkali lye, ammonium carbonate or chlorid solution, and resin-andoil mixture is pumped for about .one hour in continuous circulation through the pipe (I, filter F ,vpipe d, pump P, pipe (1 upper compartment B screen C, and lower compartment B. During this agitation the mass is continuously heated bymeans of the steamcoil'b and the steam-jacket surrounding the cooker B. Under these conditions a portion of the alkali is decomposed, liberating free the soda attacking the resin and oil.

carbonic-acid gas, which soon establishes within the circulatory system a considerable pressure. Saponification takes place, due to The increasing pressure, however, retards the decomposition of the alkali aud'soon reaches I the point when no furthersplitting up of the alkali can take place, and. as a consequence the generation of carbonic-acid gas ceases and saponification ceases likewise. The constant circulation throughthe pump produces an intimate contact of the carbonic-acid gas with the mixture, which becomes heavily charged with ca rbonic-acid gas. During the circulation the filter F removes all impurities. The object to be attained is' to render thefinal product of such a character as to be easily soluble in cold water,but without foaming, and to permit only such, saponificatiou within the cooker B as toimpart to the size this propertyin other words, to leave alarge.

This

portion of the resin in a free state. controlled during the circulation by openin more or less and at the proper times the vent-" cock I) of the cooker, so as the permit escape of carbonic acid gas. Immediately upon openingsaid vent-cock the pressure within.

the circulatory system falls, the decompositron of the alkali sets in, and additional saponification takes place, this action continuing until the-pressure again rises, due to the llberation of carbonic-acid gas,to such a point as to stop the decompositionbf the alkali. The degree of saponification and'the quality of the I P 'Oduct may by this means be controlled to a nicety. During the'mixing process herein de-; scribed the ammonium compound is also de composed. When ammonium carbonate is. used, it splits up into free ammonia and carbonic-acid gas. The ammonia attacks the resin and forms an ammonium resi'nate, while.

the carbonic-acid gas serves to increase the pressure within the circulatory system. This ammonium resinate is a valuable constituent of the product, for the reason that when pavper containing the same is dried and heated the ammonia is disengaged, leaving free resin within the paper. The'agitation having been carried on for,the period necessaryto produce the required reactions and bring the mass to the proper condition, which, asjbefore-stated, will ordinarily be about one hour, the mass is allowed to cool sufficiently so that The vent-cock b is then opened, the valve e of the pipe (1 closed, the valve e of the pipe (1 opened, and the mass pumped by a suitable pump P through the pipes d and d into the storage-tank D, from which the same maybe removed for use or sale. The proding a large percentage of free unsaponified Patent- I 1. The process. herein described of making resin size, which consists in mixing an oil or .fatwith a suitable molten resin, filtering the mixture, adding to the samea solution of an ammonium compound and an alkali lye, the :tter in suflicient quantity to induce saponi- 1n contact with carbonic-acid gas under conditions permitting saponification of only a 2. The process herein described of making resin size, whichconsists in mixing an oil .or fat with a'suitable molten resin, filtering the ammonium compound and analkali lye,.the latter in 'suffici-ent quantity to in'dtuce sap'onification, and agitating the resulting mixture such heat and pressure as to permit saponification of only a portion of the resin, sub- 'stantially as set forth.

resin,free alkali and an ammonium resinate, substantially as set forth.

In testimony whereof we have signed our two subscribing witnesses.

FRI'IZ' ARLEDTER. HERMAN ARLEDTER. Witnesses as to Fritz-Arledterz' I WALTER LANZKE, EDWARD P. MACLEAN..

Witnesses as to H.-Arledter: W. J. SULIS,

Wm. PIERCE.

. 'tion, and agitating the resulting mixtureportion of the resin, substantially as set forth.

upon exposing the same to atmospheric pres- I sure no further saponification Wlll result.

not is aresin size of superior quality, cont'ainresin, a quantity of free alkali, and a quanclaim as newand desire to secure by Letters "mixture, addingto the same a solution of in contactwith carbonic-acid gas and under 3. A resin size containing free unsaponified names to this specification'in the presence of 

